CN106398062A - Carbon nanotube-polytetrafluoroethylene valve sealing ring filled with Ti3SiC2 - Google Patents

Carbon nanotube-polytetrafluoroethylene valve sealing ring filled with Ti3SiC2 Download PDF

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Publication number
CN106398062A
CN106398062A CN201610437298.1A CN201610437298A CN106398062A CN 106398062 A CN106398062 A CN 106398062A CN 201610437298 A CN201610437298 A CN 201610437298A CN 106398062 A CN106398062 A CN 106398062A
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parts
sealing ring
sic
cnt
valve sealing
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胡光荣
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Anhui Rongda Valve Co Ltd
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Anhui Rongda Valve Co Ltd
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Priority to CN201610437298.1A priority Critical patent/CN106398062A/en
Publication of CN106398062A publication Critical patent/CN106398062A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/08—Ingredients agglomerated by treatment with a binding agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Sealing Material Composition (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a carbon nanotube-polytetrafluoroethylene valve sealing ring filled with Ti3SiC2. The valve sealing ring is prepared from the following components by weight: 100 parts of polytetrafluoroethylene, 5 to 8 parts of carbon nanotubes, 8 to 10 parts of phenol, 8 to 10 parts of p-toluylic acid, 1 to 2 parts of bentonite, 5 to 8 parts of diphenyl ether, 1 to 3 parts of butyl titanate, 20 to 25 parts of sodium hypochlorite with a concentration of 60 to 70%, 20 to 25 parts of EDTA, 40 to 50 parts of ammonia water, 80 to 100 parts of absolute ethyl alcohol, 3 to 5 parts of titanium powder, 4 to 5 parts of polycarbosilane, 18 to 20 parts of xylol, 1 to 2 parts of molybdenum disulfide, 1 to 3 parts of a silane coupling agent KH550, 9 to 10 parts of ammonium chloride, 30 to 35 parts of urea and 30 to 35 parts of water. The sealing ring disclosed by the invention has good sealing performance, better permeation resistance, wear resistance, high hardness, low creep deformation, long service life and other excellent performance.

Description

A kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling
Technical field
The invention belongs to valve sealing ring field is and in particular to a kind of Ti3SiC2Filled polytetrafluoroethylene valve sealing ring and Its preparation method and application.
Background technology
Politef（PTFE）With the chemical stability of its height, extremely strong high- and low-temperature resistance performance, prominent does not glue Property, good lubricity, excellent electrical insulating property, resistance to ag(e)ing, minimum water absorption etc. is so as in Aero-Space, oil The fields such as work, mechanical industry, electronic apparatus, food industry, weaving have a wide range of applications. but also because it has mechanical performance relatively Difference, linear expansion coefficient is big, and creep resistant is poor, and mar proof is poor, and hardness is low, and the defect such as molding and secondary operations difficulty is so as to answer It is subject to certain restrictions with scope.In order to improve and overcoming the defect of pure PTFE, frequently with surface modification, filling-modified and blending The means such as modification improving its combination property, wherein especially with filling-modified the simplest, price is low, effect is good and generally adopted With.But filler material can lead to the porous of politef, and cause variable color or pollution.
Ternary layered carbide Ti3SiC2It is uniquely real ternary compound in Ti-Si-C series, belong to hexagonal crystal system. Ti3SiC2Both there are the excellent properties of metal, such as had good heat conduction and electric conductivity in room temperature, good thermal shock resistance and Easy processing and high-temp plastic；It has the excellent properties of pottery again simultaneously, as high yield strength, high-melting-point, high heat stability Property and the high and good antioxygenic property of elevated temperature strength and decay resistance.
The present invention passes through carbon nano-tube modified with polybenzoate, then prepares Ti3SiC2Powder, finally prepares Ti3SiC2Filling Carbon nanometer-teflon valve sealing ring.Ti disclosed by the invention3SiC2The carbon nanometer of filling-teflon valve sealing Circle has a good sealing property, higher osmotic-pressure-tolerant, and the high and low creep of wear-resistant, hardness, long service life etc. are numerous excellent Performance.
Content of the invention
The primary and foremost purpose of the present invention is to provide a kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling, Carbon nanometer-teflon valve sealing ring is high temperature resistant for this, corrosion-resistant, long service life.
Another object of the present invention is to providing above-mentioned carbon nanometer-teflon valve wear-resistant, that hardness is high to seal The preparation method of circle.
A kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling is it is characterised in that described valve sealing ring It is prepared from by the component of following weight portion：100 parts of politef, CNT 5-8 part, phenol 8-10 part, to methylbenzene Formic acid 8-10 part, bentonite 1-2 part, diphenyl ether 5-8 part, butyl titanate 1-3 part, 60-70% sodium hypochlorite 20-25 part, EDTA 20-25 part, ammonia 40-50 part, dehydrated alcohol 80-100 part, titanium valve 3-5 part, Polycarbosilane 4-5 part, dimethylbenzene 18-20 part, two Molybdenum sulfide 1-2 part, silane coupler kh550 1-3 part, ammonium chloride 9-10 part, carbamide 30-35 part, water 30-35 part.
A kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling is it is characterised in that described valve sealing ring It is prepared from by following steps：
（1）CNT activation
The oxidation modification of A CNT
First molybdenum bisuphide is dispersed in 60-70% liquor natrii hypochloritises, adds CNT stirring 10-12h, sucking filtration, filter cake Put into ultrasonic 20-30min in dehydrated alcohol, 50-60 DEG C be vacuum dried 20-30h, the CNT to oxidation modification；
The activation of B CNT
The CNT of EDTA and oxidation modification is dispersed in ammonia, 50-70 DEG C, PH is ultrasonic 1-3h under the conditions of 5-7, standing 1-2h, filters, and filter cake is immersed in ultrasonic 1-3h in the mixed liquor of ammonium chloride, carbamide, water, stands 1-2h, filters, and 50-60 DEG C true Sky is dried 20-30h, to Activated Carbon Nanotubes；
（2）Polybenzoate is carbon nano-tube modified
Activated Carbon Nanotubes, phenol, P-hydroxybenzoic acid are added ultrasonic disperse 1-3h in diphenyl ether, adds catalyst metatitanic acid Butyl ester, 70-90 DEG C of esterification 8-10h, add bentonite, ultrasonic disperse 0.5-1h, improve reaction temperature and contracted to 180-200 DEG C Poly-, polycondensation 20-30h, obtain polybenzoate carbon nano-tube modified.
（3）Ti3SiC2The preparation of powder
Titanium valve and Polycarbosilane are mixed and are dissolved in organic solvent, stirring, mix homogeneously, drying；The powder low temperature dried is split Solution, temperature is 800 DEG C -1200 DEG C, temperature retention time 0.5-2h, 2-7 DEG C of programming rate/min, obtains initial reaction thing；To preliminary Reactant high-temperature process, temperature is 1400-1600 DEG C, temperature retention time 0.5-2h, 2-7 DEG C of programming rate/min；Grinding is sieved To Ti3SiC2Powder；
（4）The preparation of carbon nanometer-teflon valve sealing ring
First carry out ball milling by carbon nano-tube modified for polybenzoate, after ball milling polybenzoate carbon nano-tube modified with polyflon, Ti3SiC2After powder mixing, then silane coupler kh550 is sprayed wherein, be dried at 40～100 DEG C, the mixing that will be dried Raw material is molded in 20～60MPa chill, compression rate 5-10MPa/min pressurize 1～30min；Again the product of molding is entered Row sintering, is cooled to room temperature, that is, obtain the Ti prepared by the present invention3SiC2The carbon nanometer of filling-teflon valve sealing Circle.
Described polyflon is suspension injecting tetrafluoroethylene resin, and its particle diameter distribution is 15～60 μm；Described Ti3SiC2Powder, molybdenum bisuphide, bentonitic particle diameter are 10～50 μm；After ball milling, the carbon nano-tube modified particle diameter of polybenzoate is 10-50μm.
The Ti providing compared to other teflon valve sealing rings, the present invention3SiC2The carbon nanometer-poly- four of filling Fluorothene valve sealing ring has the excellent properties of metal, and anti-wear performance is good, high yield strength, high-melting-point, high thermal stability The antioxygenic property high and good with elevated temperature strength and decay resistance.
Specific embodiment
A kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling, by the component preparation of following weight portion Become：100 parts of politef, 5 parts of CNT, 8 parts of phenol, 10 parts of p-methylbenzoic acid, 2 parts of bentonite, 8 parts of diphenyl ether, 2 parts of butyl titanate, 22 parts of 60-70% sodium hypochlorite, 22 parts of EDTA, 40 parts of ammonia, 100 parts of dehydrated alcohol, 3 parts of titanium valve, poly- carbon 5 parts of silane, 20 parts of dimethylbenzene, 1 part of molybdenum bisuphide, 3 parts of silane coupler kh550,9 parts of ammonium chloride, 30 parts of carbamide, 30 parts of water.
A kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling, is prepared from by following steps：
（1）CNT activation
The oxidation modification of A CNT
First molybdenum bisuphide is dispersed in 70% liquor natrii hypochloritises, adds CNT stirring 10h, sucking filtration, filter cake is put into no Ultrasonic 30min in water-ethanol, 60 DEG C vacuum drying 30h, the CNT to oxidation modification；
The activation of B CNT
The CNT of EDTA and oxidation modification is dispersed in ammonia, 70 DEG C, PH is ultrasonic 1-3h under the conditions of 5, stands 2h, mistake Filter, filter cake is immersed in ultrasonic 1h in the mixed liquor of ammonium chloride, carbamide, water, stands 2h, filters, 60 DEG C of vacuum drying 20h, arrive Activated Carbon Nanotubes；
（2）Polybenzoate is carbon nano-tube modified
Activated Carbon Nanotubes, phenol, P-hydroxybenzoic acid are added ultrasonic disperse 1-3h in diphenyl ether, adds catalyst metatitanic acid Butyl ester, 75 DEG C of esterification 10h, add bentonite, ultrasonic disperse 1h, improve reaction temperature to 200 DEG C and carry out polycondensation, polycondensation 30h, obtain Carbon nano-tube modified to polybenzoate.
（3）Ti3SiC2The preparation of powder
Titanium valve and Polycarbosilane are mixed and are dissolved in organic solvent, stirring, mix homogeneously, drying；The powder low temperature dried is split Solution, temperature is 1000 DEG C, temperature retention time 2h, 2-7 DEG C of programming rate/min, obtains initial reaction thing；To initial reaction thing high temperature Process, temperature is 1400 DEG C, temperature retention time 0.5-2h, 5 DEG C/min of programming rate；Grind screening and obtain Ti3SiC2Powder；
（4）The preparation of carbon nanometer-teflon valve sealing ring
First carry out ball milling by carbon nano-tube modified for polybenzoate, after ball milling polybenzoate carbon nano-tube modified with polyflon, Ti3SiC2After powder mixing, then silane coupler kh550 is sprayed wherein, be dried at 70 DEG C, the mixed material that will be dried Molded in 50MPa chill, compression rate 8MPa/min pressurize 30min；Again the product of molding is sintered, is cooled to room Temperature, that is, obtain Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling.
After tested：Draw high intensity 27MPa；Elongation at break 210%；Impact strength 22.5KJ/m；Bending strength 27MPa；Mill Consumption 4.2mm3（Load 250N, linear velocity 2m/s, 3 minutes time）.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and any Those of ordinary skill in the art disclosed herein technical scope in, the change that can expect without creative work or Replace, all should be included within the scope of the present invention.Therefore, protection scope of the present invention should be limited with claims Fixed protection domain is defined.

Claims (3)

1. a kind of Ti3SiC2Filling carbon nanometer-teflon valve sealing ring it is characterised in that described valve sealing ring by The component of following weight portion is prepared from：100 parts of politef, CNT 5-8 part, phenol 8-10 part, to methylbenzene first Sour 8-10 part, bentonite 1-2 part, diphenyl ether 5-8 part, butyl titanate 1-3 part, 60-70% sodium hypochlorite 20-25 part, EDTA 20- 25 parts, ammonia 40-50 part, dehydrated alcohol 80-100 part, titanium valve 3-5 part, Polycarbosilane 4-5 part, dimethylbenzene 18-20 part, two sulfur Change molybdenum 1-2 part, silane coupler kh550 1-3 part, ammonium chloride 9-10 part, carbamide 30-35 part, water 30-35 part.
2. a kind of Ti3SiC2Filling carbon nanometer-teflon valve sealing ring it is characterised in that described valve sealing ring by Following steps are prepared from：
CNT activation
The oxidation modification of A CNT
First molybdenum bisuphide is dispersed in 60-70% liquor natrii hypochloritises, adds CNT stirring 10-12h, sucking filtration, filter cake Put into ultrasonic 20-30min in dehydrated alcohol, 50-60 DEG C be vacuum dried 20-30h, the CNT to oxidation modification；
The activation of B CNT
The CNT of EDTA and oxidation modification is dispersed in ammonia, 50-70 DEG C, PH is ultrasonic 1-3h under the conditions of 5-7, standing 1-2h, filters, and filter cake is immersed in ultrasonic 1-3h in the mixed liquor of ammonium chloride, carbamide, water, stands 1-2h, filters, and 50-60 DEG C true Sky is dried 20-30h, to Activated Carbon Nanotubes；
Polybenzoate is carbon nano-tube modified
Activated Carbon Nanotubes, phenol, P-hydroxybenzoic acid are added ultrasonic disperse 1-3h in diphenyl ether, adds catalyst metatitanic acid Butyl ester, 70-90 DEG C of esterification 8-10h, add bentonite, ultrasonic disperse 0.5-1h, improve reaction temperature and contracted to 180-200 DEG C Poly-, polycondensation 20-30h, obtain polybenzoate carbon nano-tube modified；
Ti3SiC2The preparation of powder
Titanium valve and Polycarbosilane are mixed and are dissolved in organic solvent, stirring, mix homogeneously, drying；The powder low temperature dried is split Solution, temperature is 800 DEG C -1200 DEG C, temperature retention time 0.5-2h, 2-7 DEG C of programming rate/min, obtains initial reaction thing；To preliminary Reactant high-temperature process, temperature is 1400-1600 DEG C, temperature retention time 0.5-2h, 2-7 DEG C of programming rate/min；Grinding is sieved To Ti3SiC2Powder；
The preparation of carbon nanometer-teflon valve sealing ring
First carry out ball milling by carbon nano-tube modified for polybenzoate, after ball milling polybenzoate carbon nano-tube modified with polyflon, Ti3SiC2After powder mixing, then silane coupler kh550 is sprayed wherein, be dried at 40～100 DEG C, the mixing that will be dried Raw material is molded in 20～60MPa chill, compression rate 5-10MPa/min pressurize 1～30min；Again the product of molding is entered Row sintering, is cooled to room temperature, that is, obtain the Ti prepared by the present invention3SiC2The carbon nanometer of filling-teflon valve sealing Circle.
3. a kind of Ti3SiC2Carbon nanometer-teflon valve the sealing ring of filling is it is characterised in that described politef tree Fat is suspension injecting tetrafluoroethylene resin, and its particle diameter distribution is 15～60 μm；Described Ti3SiC2Powder, molybdenum bisuphide, bentonitic Particle diameter is 10～50 μm；After ball milling, the carbon nano-tube modified particle diameter of polybenzoate is 10-50 μm.
CN201610437298.1A 2016-06-20 2016-06-20 Carbon nanotube-polytetrafluoroethylene valve sealing ring filled with Ti3SiC2 Withdrawn CN106398062A (en)

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CN201610437298.1A CN106398062A (en) 2016-06-20 2016-06-20 Carbon nanotube-polytetrafluoroethylene valve sealing ring filled with Ti3SiC2

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108546467A (en) * 2018-04-19 2018-09-18 厦门富思特新材料科技有限公司 A kind of high hardness wear-resisting aqueous wooden ware solid color enamel and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102050448A (en) * 2009-11-06 2011-05-11 中国科学院上海硅酸盐研究所 Method for preparing Ti3SiC2-based powder
CN102492157A (en) * 2011-12-07 2012-06-13 江苏梅兰化工有限公司 Preparation method for dispersed graphite filled polytetrafluoroethylene resin
CN102174248B (en) * 2011-03-28 2012-10-03 上海交通大学 Method for preparing carbon nanotube/polybenzoate composite
CN102952360A (en) * 2012-11-06 2013-03-06 浙江国威汽车配件有限公司 Fluorine-containing polymer mixing material and method for preparing bulb buffer ball keyway by same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102050448A (en) * 2009-11-06 2011-05-11 中国科学院上海硅酸盐研究所 Method for preparing Ti3SiC2-based powder
CN102174248B (en) * 2011-03-28 2012-10-03 上海交通大学 Method for preparing carbon nanotube/polybenzoate composite
CN102492157A (en) * 2011-12-07 2012-06-13 江苏梅兰化工有限公司 Preparation method for dispersed graphite filled polytetrafluoroethylene resin
CN102952360A (en) * 2012-11-06 2013-03-06 浙江国威汽车配件有限公司 Fluorine-containing polymer mixing material and method for preparing bulb buffer ball keyway by same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108546467A (en) * 2018-04-19 2018-09-18 厦门富思特新材料科技有限公司 A kind of high hardness wear-resisting aqueous wooden ware solid color enamel and preparation method thereof
CN108546467B (en) * 2018-04-19 2021-06-04 厦门富思特新材料科技有限公司 High-hardness wear-resistant water-based woodware solid-color paint and preparation method thereof

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Application publication date: 20170215